Process for fibrillating lignocellulosic material, fibres and their use
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example 1
Preparation of 1-methyl-3-methylimidazolium dimethylphosphate ([mmim]Me2PO4)
[0070]A mixture of 1-methylimidazole (50 ml, 0.519 mol) was added over a space of 4 hrs to trimethylphosphate (60.7 ml, 0.519 mol) at 100° C., with stirring. The solution was heated at 100° C. for a further 18 hrs. The reaction of the mixture was determined to be complete by analyzing a sample by 1H NMR from CDCl3. The mixture was rotary evaporated under high vacuum for 18 hrs to give a pale yellow oily product (110 ml). The purity of the product was determined to be >99% by 1H NMR analysis.
example 2
Preparation of 1-ethyl-3-methylimidazolium dimethylphosphate ([emim]Me2PO4)
[0071]A mixture of 1-ethylimidazole (50 ml, 0.519 mol) was added over a space of 4 hrs to trimethylphosphate (60.7 ml, 0.519 mol) at 120° C. with stirring. The solution was heated at 120° C. for a further 18 hrs. The reaction of the mixture was determined to be complete by analyzing a sample by 1H NMR from CDCl3. The mixture was rotary evaporated under high vacuum for 18 hrs to give a pale yellow oily product (110 ml). The purity of the product was determined to be >99% by 1H NMR analysis.
example 3
Preparation of 1-ethyl-3-methylimidazolium methylhydrogenphosphonate ([emim]MeHPO3)
[0072]A mixture of 1-ethylimidazole (50 ml, 0.519 mol) was added over a space of 4 hrs to diethylphosphite (47.6 ml, 0.519 mol) at 140° C. with stirring. The solution was heated at 140° C. for a further 18 hrs. The reaction of the mixture was determined to be complete by analyzing a sample by 1H NMR from CDCl3. The mixture was rotary evaporated under high vacuum for 18 hrs to give a pale yellow oily product (97 ml). The purity of the product was determined to be >99% by 1H NMR analysis.
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